Reaktionsgleichung
[C:1]1([CH:8]=[CH:7][C:5]([OH:6])=[CH:4][CH:3]=1)[OH:2].CCCCCCC.[S:16](=O)(=[O:19])([OH:18])[OH:17].C(C(CCCC)C([O-])=O)C.[K+:31]>C(OCC)(=O)C>[K+:31].[OH:2][C:1]1[CH:8]=[CH:7][C:5]([OH:6])=[CH:4][C:3]=1[S:16]([O-:19])(=[O:18])=[O:17]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 12.5 °C
Versuchsvorschrift
Hydroquinone (20 g, 0.1816 mol) and n-heptane (60 mL) was taken in a round bottom flask, after cooling the flask to about 10-15° C., sulfuric acid (36 N, 17.8 g) was added dropwise at the same temperature and stirring continued further for about 10-15 min. The temperature was slowly raised to 50-60° C. then stirred for 3-8 h. The reaction mass was then cooled to 25-35° C., n-heptane was decanted and ethyl acetate (200 mL) added to dissolve the solid formed. A solution of potassium 2-ethylhexanoate (36.4 g, 0.1996 mol) in ethyl acetate (200 mL) was added slowly. The reaction was further stirred for an hour. The precipitated crude solid was filtered, washed with ethyl acetate to give 40 g of 2,5-dihydroxybenzenesulfonic acid potassium salt.
Aufarbeitung
- temperatureThe temperature was slowly raised to 50-60° C.
- stirringthen stirred for 3-8 h
- temperatureThe reaction mass was then cooled to 25-35° C.
- customn-heptane was decanted
- additionethyl acetate (200 mL) added
- dissolutionto dissolve the solid
- customformed
- stirringThe reaction was further stirred for an hour
- customThe precipitated crude solid
- filtrationwas filtered
- washwashed with ethyl acetate
Quellen und Nachweise
- ORD-Eintrag
- ord-f2e3b518a908402e83ccb91b631e39bc
- Quelldatensatz
- uspto-grants-2016_01
- Patentnummer
- US09227928B2
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